溶剂吸收-GC/MS联用测定蔬菜中二硫代氨基甲酸酯类杀菌剂  

Determination of Dithiocarbamate Fungicides in Vegetables by Solvent Absorption-GC/MS

作　　者：马淑青[1] 代飞飞[1] MA Shuqing;DAI Feifei(Weifang District Center for Disease Control and Prevention,Weifang 261061,China)

机构地区：[1]潍坊市疾病预防控制中心,山东潍坊261061

出　　处：《食品安全导刊》2022年第16期108-110,共3页China Food Safety Magazine

基　　金：潍坊市卫健委科研项目(wfwsjs_2018_051)。

摘　　要：目的:通过优化气相色谱和质谱条件,建立溶剂吸收结合气相色谱-质谱法测定蔬菜中二硫代氨基甲酸酯类杀菌剂的方法。方法:样本中的二硫代氨基甲酸盐(酯)类杀菌剂在加热的密闭顶空瓶中,遇氯化亚锡-盐酸溶液时,消化反应生成二硫化碳,冷却后用正己烷萃取出二硫化碳,气相色谱质谱测定正己烷相中二硫化碳的量,用以代表二硫代氨基甲酸酯类杀菌剂的残留量。结果:高、低浓度标准系列相关系数均大于0.998,检出限为0.006 mg/kg,平均加标回收率在84.0%~93.4%,相对标准偏差为4.5%~10.8%。结论:所建立的方法简便、快速,具有较高的准确度与精密度,净化效果好,回收率高,可用于蔬菜中二硫代氨基甲酸酯类杀菌剂的测定。Objective:A method for the determination of dithiocarbamate fungicides in vegetables by solvent absorption combined with gas chromatography-mass spectrometry was established by optimizing the conditions of gas chromatography and mass spectrometry.Method:In the heated closed headspace bottle,the dithiocarbamates(DTCs)were digested into carbon disulfide gas by HCl/SnCl_(2) solution.After cooling down,carbon disulfide was absorbed by hexane solution,and then determined by gas chromatography-mass spectrometry to be quantified,thus representing the residual level of DTCs pesticide residues.Result:The correlation coefficients for high and low concentration standards were all higher than 0.998.The minimum detection concentration was 0.006 mg/kg.The average recovery rates were in a range from 84.0%to 93.4%.The relative standard deviations were in a range from 4.5%to 10.8%.Conclusion:This established method is simple,rapid with high accuracy and precision good purification effect and high recovery.It can be used for the determination of dithiocarbamate fungicides in vegetables.

关 键 词：二硫代氨基甲酸酯 气相色谱-质谱(GC-MS) 蔬菜 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]